Process of purifying monochlorhydrin.



UNITED STATES PATENT OFFICE.

FRIEDRICH CARL HEYEIR, OF SCHLEIBUSCH-MANFORT, GERMANY," ASSIGNOR T0 E. I.

DU PONT DE NEMOURS POWDER. COMPANY, OF WILMINGTON, DELAWARE, A CORPO- RATION OF NEW JERSEY.

PROCESS, OF PURIFYIN G MONOCHLORHYDRIN.

No Drawing.

PatentedOct. 8,1912.

To all whom it may concur-n:

'Be it known that I, FRIEDRICH CARL Hanan, a subject of the Emperor of Germany, residing at Schlebusch-Manfort, Germany, have invented a new and useful Improvement in Processes of Purifying Mono may be separated from the glycerin by frac-.

tional distillation. It is found advanta- .geous to=further purify the chlorinated material beforenitrating or distillingthe same and to effect the removal of the resinificatiop products and other impuritiesthat have been produced. .This urification' may be accomplished toa vsutlicient degree by treating the chlorinated material with animal charcoal or with similar substances, but thls method is objectionable because of both its inconvenience-and its expense. It has also been attempted to free the chlorinated material from the separated sulfur by pressing or by suctional filtration, or by filtering the same otherwise and obtaining the remainder by washing the sulfur with hot water. As the sulfur is obtained in granular form containing lumps as large as hens eggs, it is necessary to finely pulverize the sulfur before it is washed. Notwithstandlng this, a complete separation of the chlorinated material bythe above method is very diflicult,

and the sulfur available is not sufficiently pure to render its direct use possible, as it contains Water,-residues. of the chlorinated I material, resins, sulfur oils, etc, in quantities as high as fifteen .per cent. The objects of my invention are: First, to substantially free the chlorinated material ,from the byroducts that it contains by convenient an inexpensive means; and second, to substantially free the separated sulfur from impurities arid permit. it to beused directly and at the same time to completely separate therefrom the chlorinated material.

In carrying out my invention, I dilute the crude chlorinated product with water, preferably about two volumes of water to one volume of the chlorinated product, then per mit the resins, sulfur, etc, to settle and remove the same, or separate the same by filtration, then if desired) decolorize the clear liquid thus obtained by means of animal charcoal or other similar substances, and then concentrate the same for a prolonged tlme in a vacuum at a temperature of from 40 to 100 C. toliberate the clear liquid from water, hydrochloric acid, dichlorhydrin and other impurities that are present in solution. It will be understood that the removal of the solid materials by filtration and their removal by settlement arc equivalent steps, and that in specifying one step in the claims, I do not mean to exclude the other step as an equivalent.

The separated sulfur, together with the 'chlorlnated material adhering to same, are heated to a temperature of about 120 C.

-The sulfur melts and the chlorinated material which possesses a lower specific gravity, rises to the top, and can be either skimmed off or allowed to flow off into a separate receptacle. The sulfur thus obtained is free from water and contains only small quantities of organic impurities. The separated chlorinatedmaterial thus obtained may be purified in the same manner as the .bulk of the product.

The degree of vacuum employed is about 70 mm. It is not desirable to work with a pressure higher than 60-70 mm. on account of the higher temperature. The lowest possible pressure is the most fiective. The time required for vaporizati is about sixteen hours for 100 kg. of the finished product, but the time will vary with the apparatus and method of operation employed. The preferred density. of the evaporated liquid is 1.10 to Lil-13 to 15 Be. v

If it is desired to decolorize (whichis no essential feature of my process in its broadestaspect) the liquid liberated from the bulk of the dissolved resins by means of dilution is diluted with not less than 12% animal charcoal, heated for about one-half hour under stirring to about 70, permitted to stand for some little time and is then later filtered. The animal charcoal is, depending'upon its quality, treated preliminarily.

, Patent is v 1. The process of purifying the chlorinated product obtained bythe action of chlorinated sulfur upon glycerin, which consists in diluting the same with water, removing the sulfur and other material that may be removed'by filtration, and then removing the' water, hydrochloric acid and dichlorhydrin by subjecting the clear liquid thus obtained to prolonged heating in a vacuum at a temperature of between 40 and 100C.

2. The process of purifying the chlorinated product obtained by the action of chlorinated sulfur upon glycerin, which consists 1 1n diluting the same with water, removing the sulfur and other materials that may be removed by filtration, decolorizing .the clear liqu d thus obtained and subjecting it to prolonged heating in a vacuum at a temperature of between 40 and 100 C.

3. The process of purifying the chlorinated product obtained by the action of chlorinated sulfur upon glycerin, consists, in diluting said product with water, removing the sulfur and other materials that may be the sulfur and the chlorinated material adhering thereto to a temperature sufficiently high to "melt the sulfur, removing the. chlorinated material which is separated above the molten sulfur, and subjecting the clear liquid remaining after removal of the sulfur, and also. the chlorinated material separated from the sulfur,

to prolonged heating in a vacuum at a temperature between 40 and 100 0.," thereby removing water, hydrochloric acid, and dichlorhydrin;

In testimony of which invention, I have hereunto set my hand, at Cologne, on this 22'day of April, 1910. v

FRIEDRTGH CARL HEYER.

Witnesses:

JAcoB VON HERKEN, T. G, FRITZ EMoNs.

which removed by filtration, heating 

